反应详情

温度

50 °C

To a solution of 9-chloro-1-(2,4-dichlorophenyl)-1,2,3,4-tetrahydropyrimido[1,2-a]benzimidazole-6-carbonitrile (1.496 g, 3.096 mmol) in tetrahydrofuran (40 mL) was added ethylmagnesium bromide (3.0 M solution in diethyl ether, 13.2 mL, 39.6 mmol) at 0° C. The reaction mixture was stirred at 50° C. for 4 hr, then the mixture was cooled to room temperature. A suspension of sodium tetrahydroborate (3.0 g, 79.3 mmol) in 2-propanol (40 mL) was added to the reaction mixture at room temperature. After the mixture was stirred at room temperature for 18 hr, water was added to the reaction mixture at 0° C. The mixture was extracted with ethyl acetate. The organic layer was washed with water and brine, dried over anhydrous magnesium sulfate, concentrated in vacuo to give title compound (1.68 g) as a pale yellow amorphous.

1. temperaturethe mixture was cooled to room temperature
2. additionwas added to the reaction mixture at room temperature
3. stirringAfter the mixture was stirred at room temperature for 18 hr
4. extractionThe mixture was extracted with ethyl acetate
5. washThe organic layer was washed with water and brine
6. dry with materialdried over anhydrous magnesium sulfate
7. concentrationconcentrated in vacuo